化工社化工社 化学情報印刷レポート · 研究参考用
Nitric Acid → Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pnu-288034 | HCID 9931003 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide | HCID 9922094 | 94.2% |
反応手順
To a suspension of the product of example 1 (300 g, 1.21 mol) in 3 L of acetic acid, nitric acid (255 mL, ca. 6 mol, fuming, 90%) is added over 30 min at room temperature. Yellow precipitate is formed within minutes and increases over time. The reaction is kept at room temperature for 18 hours, before it is poured into 6 L of water. After stirred for 2 hours, the yellow suspension is filtered. The precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2) and dried in oven at 50° C. overnight to give 333 g (94%) of the title compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06605609B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-005797f02363405c9b410f8b0a949391 |
| 出典メモ | uspto-grants-2003_08 |